CN113087086B - Carbon plate electrode based on waste pine residue and preparation method thereof - Google Patents

Carbon plate electrode based on waste pine residue and preparation method thereof Download PDF

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Publication number
CN113087086B
CN113087086B CN202110331189.2A CN202110331189A CN113087086B CN 113087086 B CN113087086 B CN 113087086B CN 202110331189 A CN202110331189 A CN 202110331189A CN 113087086 B CN113087086 B CN 113087086B
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carbon plate
plate electrode
residue
water
carbon
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CN113087086A (en
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景江
白世星
陈辣
倪家明
张欣
何思雨
范天斌
王卓
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Chengdu Technological University CDTU
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C02F2001/46138—Electrodes comprising a substrate and a coating
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical

Abstract

The invention discloses a carbon plate electrode based on waste pine residue and a preparation method thereof, belonging to the technical field of electrochemistry,the porous carbon is generated by uniformly mixing the porous carbon with water filled with micro-nano bubbles, so that the micro-nano bubbles occupy the internal space of pine residue, and a porous space is formed in the pine residue, so that the space channel of the final carbon plate electrode material is greatly expanded, and the reaction efficiency is greatly improved; performing high-temperature carbonization treatment twice and combining alternate treatment of alkaline solution and acidic solution to prepare the carbon plate electrode material with micro-nano holes; the carbon plate electrode material can be used as a cathode electrode in an electrochemical device by adding H 2 O and O 2 Reduction to H 2 O 2 ，H 2 O 2 Decomposing into hydroxyl free radical to complete the sewage treatment process. The invention can effectively solve the problems of low reaction efficiency and high cost of the existing carbon electrode material.

Description

Carbon plate electrode based on waste pine residue and preparation method thereof
Technical Field
The invention relates to the technical field of electrochemistry, in particular to a carbon plate electrode based on waste pine residue and a preparation method thereof.
Background
With the rapid development of industry, the variety and quantity of wastewater are rapidly increased, and the pollution to water bodies is also becoming wide and serious day by day, threatening the health and safety of human beings. In recent years, with the rapid development of the power industry, electrochemical sewage treatment technology is applied to the field of power. Compared with other wastewater treatment methods, the electrochemical water treatment method has attracted attention at home and abroad due to the advantages of the electrochemical water treatment technology. With the development of electrode materials, the development of reactors and the improvement of the traditional electrochemical process, the electrochemical water treatment technology as a clean treatment process is bound to be more widely applied.
The electrochemical water treatment technology is a technical process which is characterized in that a large number of free radicals are generated through a series of designed chemical reactions, electrochemical processes or physical processes in a specific electrochemical reaction device under the action of an external electric field, and then pollutants in wastewater are degraded by utilizing the strong oxidizing property of the free radicals, and is one of advanced oxidation technologies. However, the electrode material of the existing electrochemical reaction device mainly has the following two problems: 1) The conventional carbon electrode material has too low surface area, so that the reaction efficiency is low and the sewage treatment effect is poor; 2) Although the metal-doped carbon electrode material has good reaction efficiency, the manufacturing cost is high, and the further application of the metal-doped carbon electrode material is limited. Therefore, it is very significant to provide a carbon plate electrode with high reaction efficiency and low cost.
Disclosure of Invention
Aiming at the defects or shortcomings, the invention aims to provide a carbon plate electrode based on waste pine residue and a preparation method thereof, which can effectively solve the problems of low reaction efficiency and high cost of the existing carbon electrode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a carbon plate electrode based on waste pine residue, which specifically comprises the following steps:
step (1): uniformly stirring and mixing the water filled with the micro-nano bubbles and the waste pine wood residues, standing for 60-80 min, drying, and performing rolling forming to prepare a carbon plate; wherein the mass ratio of water to the waste pine residue is 1-2.
Step (2): performing first carbonization treatment on the carbon plate obtained in the step (1) in a nitrogen atmosphere, then immersing the carbon plate into an alkaline solution for 5-7 hours, taking out the carbon plate and drying the carbon plate, performing second carbonization treatment in the nitrogen atmosphere, then washing the surface of the carbon plate to be neutral through an acidic solution and clear water, and drying to obtain a porous carbon plate;
and (3): and (3) coating the two surfaces of the porous carbon plate obtained in the step (2) with epoxy resin glue to form an electrode shape, reserving a lead position on one surface of the porous carbon plate, and sealing other planes by using the epoxy resin glue to obtain the carbon plate electrode.
Furthermore, the particle size of the waste pine wood residue in the step (1) is 20-60 meshes.
Further, the mass ratio of the water to the waste pine wood residues in the step (1) is 1.
Further, the temperature of the first carbonization treatment and the second carbonization treatment in the step (2) is 900-1100 ℃, and preferably 900 ℃; the first carbonization treatment time is 3 to 5 hours, preferably 3 hours; the time for the second carbonization treatment is 1 to 3 hours, preferably 1 hour.
Further, the alkaline solution in the step (2) is a sodium hydroxide aqueous solution with the molar concentration of 1.0-3.0 mol/L; the molar concentration of the aqueous sodium hydroxide solution is preferably 1.0mol/L.
Further, the acid solution in the step (2) is hydrochloric acid water solution with the molar concentration of 0.5-1.5 mol/L; the molar concentration of the aqueous hydrochloric acid solution is preferably 0.5mol/L.
Further, the epoxy resin glue in the step (3) is prepared by mixing epoxy resin and water according to the mass ratio of 1-3; the mass ratio of the epoxy resin to the water is preferably 3.
Furthermore, the epoxy resin in the epoxy resin adhesive is bisphenol A epoxy resin.
Further, the shape of the electrode in step (3) is rectangular, preferably square.
The invention also provides a carbon plate electrode prepared by the preparation method of the carbon plate electrode based on the waste pine residues.
The invention also provides an electrochemical sewage treatment device, wherein the cathode electrode of the electrochemical sewage treatment device is the carbon plate electrode.
Furthermore, the electrochemical sewage treatment device also comprises a reaction tank, a baffle is fixedly arranged in the reaction tank, magnetic generating electric rollers and carbon plate electrodes are respectively arranged on two sides of the baffle, a water flow channel is arranged in the middle of the baffle, the magnetic generating electric rollers and the carbon plate electrodes are connected through a lead, the reaction tank is provided with an aeration device, and a water inlet and a water outlet are respectively arranged on two sides of the reaction tank.
Furthermore, the aeration device comprises a micropore air dispersion disc positioned at the bottom of the reaction tank, and the micropore air dispersion disc is communicated with the blower.
The invention has the following advantages:
1. the invention provides a carbon plate electrode based on waste pine residue and a preparation method thereof, wherein the waste pine residue is used as a raw material and is uniformly mixed with water filled with micro-nano bubbles, so that the micro-nano bubbles occupy the internal space of the pine residue, a porous space is manufactured in the pine residue, porous carbon is generated, the space channel of the final carbon plate electrode material is greatly expanded, and the reaction efficiency is greatly improved; performing high-temperature carbonization treatment twice and combining alternate treatment of alkaline solution and acidic solution to prepare the carbon plate electrode material with micro-nano holes; after carbonization treatment, the carbon plate electrode is more durable and the porosity is further improved, and the porous material is neutral by treatment of the alkaline solution and the acidic solution, so that the reaction rate of the carbon plate electrode material can be improved, and the sewage removal effect of the carbon plate electrode is improved; the whole carbon plate electrode has low manufacturing cost and can be used for generating H in an electrochemical device 2 O and O 2 Reduction to H 2 O 2 ，H 2 O 2 The compound is decomposed into hydroxyl free radicals, and has practical application value in the field of sewage treatment;
2. the invention provides an electrochemical sewage treatment device using the carbon plate electrode as a cathode electrode, wherein sewage to be treated containing organic matters and harmful substances (bacteria, fungi and viruses) is introduced into a reaction tank, the sewage drives a magnetic generating roller to generate current, the current flows into the carbon plate electrode through a lead, reduction reaction occurs on the carbon plate electrode, reduction reaction occurs when water flow and oxygen reach one electrode of the carbon plate, and H is converted into H 2 O and O 2 Reduction to H 2 O 2 ，H 2 O 2 Decomposing the wastewater into hydroxyl free radicals, wherein the hydroxyl free radicals have the functions of degrading organic matters and decomposing harmful substances to complete the wastewater treatment process; the electrochemical sewage treatment device can efficiently degrade macromolecular substances, bacteria and other harmful substances in sewage.
Drawings
FIG. 1 is a schematic view of a carbon plate electrode in example 1 of the present invention;
FIG. 2 is a schematic view of an electrochemical sewage treatment apparatus according to example 1 of the present invention;
wherein, 1, a reaction tank; 2. a magnetically generating roller; 3. a baffle plate; 4. a wire; 5. a carbon plate electrode; 6. an aeration device.
Detailed Description
Example 1
The embodiment 1 provides a carbon plate electrode based on waste pine residue and a preparation method thereof, and specifically comprises the following steps:
step (1): firstly, a large amount of bubbles are injected into deionized water through a micro-nano bubble generator, water filled with micro-nano bubbles and waste pine wood residues are stirred and mixed uniformly, the mixture is kept stand for 60min, and then the mixture is dried at the temperature of 80 ℃ for 60min and rolled under the pressure of 5000N to form a carbon plate; wherein, the mass ratio of water to waste pine wood residue is 1, the particle size of the waste pine wood residue is 20-60 meshes, and the size of the carbon plate in the embodiment 1 is 40cm by 5cm;
step (2): carbonizing the carbon plate obtained in the step (1) at 900 ℃ for 3 hours in a nitrogen atmosphere; then immersing the carbon plate into 1.0mol/L sodium hydroxide aqueous solution for 5 hours, taking out the carbon plate, drying at the temperature of 80 ℃ for 60 minutes, placing the carbon plate in a nitrogen atmosphere after drying, carbonizing at the temperature of 900 ℃ for 1 hour, washing the surface of the carbon plate to be neutral by using 0.5mol/L hydrochloric acid aqueous solution and a large amount of high-purity water, and drying at the temperature of 80 ℃ for 120 minutes to obtain the porous carbon plate;
and (3): coating 20ml of epoxy resin adhesive on two surfaces of the porous carbon plate obtained in the step (2) to form a square of 2cm x 2cm, wherein the line width of the square is 0.5cm, reserving a lead position on one surface of the porous carbon plate, and sealing other planes by using the epoxy resin adhesive to obtain a 2cm x 2cm carbon plate electrode, wherein the carbon plate electrode is shown in figure 1; the epoxy resin adhesive is prepared by mixing bisphenol A epoxy resin and water according to a mass ratio of 3.
The embodiment 1 further provides an electrochemical sewage treatment device using the carbon plate electrode as a cathode electrode, as shown in fig. 2, the electrochemical sewage treatment device specifically includes a reaction tank 1, a baffle 3 is fixedly arranged in the reaction tank 1, two sides of the baffle 3 are respectively provided with a magnetic generation electric roller 2 and a carbon plate electrode 5, a water flow channel is arranged in the middle of the baffle 3, the magnetic generation electric roller 2 and the carbon plate electrode 5 are connected through a wire 4, the reaction tank 1 is provided with an aeration device 6, the aeration device 6 includes a microporous gas diffusion disc located at the bottom of the reaction tank 1, the microporous gas diffusion disc is communicated with an air blower, and two sides of the reaction tank 1 are respectively provided with a water inlet and a water outlet.
Example 2
This example 2 provides a carbon plate electrode based on waste pine residue and a method for preparing the same, which are different from those of example 1 only in that: the mass ratio of the water to the waste pine wood residues in the step (1) is 1.
Example 2 also provides an electrochemical wastewater treatment apparatus using the carbon plate electrode as a cathode electrode, which is different from example 1 only in that: the carbon plate electrode prepared in example 1 was replaced with the carbon plate electrode prepared in example 2.
Example 3
This example 3 provides a carbon plate electrode based on waste pine residue and a method for preparing the same, which are different from those of example 1 only in that: the mass ratio of the water to the waste pine residue in the step (1) is 2.
Example 3 also provides an electrochemical wastewater treatment apparatus using the carbon plate electrode as a cathode electrode, which is different from example 1 only in that: the carbon plate electrode prepared in example 1 was replaced with the carbon plate electrode prepared in example 3.
Comparative example 1
The comparative example 1 provides a carbon plate electrode based on waste pine residue and a preparation method thereof, and the difference from the example 1 is only that: in the step (2), the surface of the carbon plate was washed with 0.5mol/L hydrochloric acid aqueous solution to acidity (pH = 3), and the rest of the steps and parameters were the same.
This comparative example 1 also provides an electrochemical sewage treatment apparatus using the above-described carbon plate electrode as a cathode electrode, differing from example 1 only in that: the carbon plate electrode prepared in example 1 was replaced with the carbon plate electrode prepared in comparative example 1.
Comparative example 2
The comparative example 2 provides a carbon plate electrode based on waste pine residue and a preparation method thereof, and only differs from the example 1 in that: in the step (2), the surface of the carbon plate is washed with 0.5mol/L hydrochloric acid aqueous solution until the carbon plate is weakly alkaline (pH = 8.5), and the rest steps and parameters are the same.
This comparative example 2 also provides an electrochemical sewage treatment apparatus using the above-described carbon plate electrode as a cathode electrode, differing from example 1 only in that: the carbon plate electrode prepared in example 1 was replaced with the carbon plate electrode prepared in comparative example 2.
Examples of the experiments
In this experimental example 1, the electrochemical wastewater treatment apparatuses described in example 1 and comparative examples 1 to 2 were used to examine the wastewater treatment capabilities of the carbon plate electrode and the electrochemical wastewater treatment apparatus provided by the present invention. Sewage to be treated in a certain hospital (inlet water amount: 500 m) 3 The water quality is as follows: ρ (COD) =359mg/L, ρ (BOD) =201mg/L, and the number of coliform groups =2.6 × 10 7 MPN/L, pH = 6-7. The sewage enters the electrochemical sewage treatment device in the embodiment 1 and runs for 120 minutes, and the running conditions are as follows: wet to dry ratio 1:3, ambient temperature 18-35 ℃, inflow rate 4.0mL/min (experiment set 1), 5.5mL/min (experiment set 2), and 7.0mL/min (experiment set 3). The results of the running experiments are shown in table 1.
TABLE 1 Hospital wastewater 120min treatment results
Figure BDA0002994535070000071
As can be seen from table 1, the electrochemical sewage treatment device provided in embodiment 1 of the present invention can efficiently degrade high molecular substances in hospital sewage and remove harmful substances such as coliform bacteria, and has a COD removal rate of up to 87% and a BOD removal rate of up to 92%, and meets the discharge standard of "discharge standard of water pollutants for medical institutions" (GB 18466-2005); while the average removal rates of COD and BOD in comparative examples 1-2 were 68% and 73% and 70% and 80%, respectively, which indicates that the carbon plate electrode fabricated using the porous carbon plate fabricated under acidic or alkaline conditions may decrease the sewage treatment capacity of the electrochemical sewage treatment apparatus.
The foregoing is merely exemplary and illustrative of the present invention and it is within the purview of one skilled in the art to modify or supplement the embodiments described or to substitute similar ones without the exercise of inventive faculty, and still fall within the scope of the claims.

Claims (7)

1. A preparation method of a carbon plate electrode based on waste pine residue is characterized by comprising the following steps:
step (1): uniformly stirring and mixing the water filled with the micro-nano bubbles and the waste pine wood residues, standing for 60-80 min, drying, and performing rolling forming to prepare a carbon plate; wherein the mass ratio of water to the waste pine residue is 1-2;
step (2): performing primary carbonization treatment on the carbon plate obtained in the step (1) in a nitrogen atmosphere, then immersing the carbon plate into an alkaline solution for 5-7 hours, taking out the carbon plate and drying the carbon plate, performing secondary carbonization treatment in the nitrogen atmosphere, finally washing the surface of the carbon plate to be neutral through an acidic solution and clear water, and drying to obtain a porous carbon plate;
and (3): coating the two surfaces of the porous carbon plate obtained in the step (2) with epoxy resin glue to form electrode shapes, reserving a lead position on one surface of the porous carbon plate, and sealing other planes with the epoxy resin glue to obtain a carbon plate electrode;
the particle size of the waste pine wood residue in the step (1) is 20-60 meshes; the mass ratio of the water to the waste pine residue in the step (1) is 1; the temperature of the first carbonization treatment and the second carbonization treatment in the step (2) is 900-1100 ℃, the time of the first carbonization treatment is 3-5 hours, and the time of the second carbonization treatment is 1-3 hours.
2. The method for preparing a carbon plate electrode based on waste pine wood residues as claimed in claim 1, wherein the alkaline solution in the step (2) is an aqueous sodium hydroxide solution having a molar concentration of 1.0 to 3.0mol/L, and the acidic solution is an aqueous hydrochloric acid solution having a molar concentration of 0.5 to 1.5 mol/L.
3. The method for preparing a carbon plate electrode based on waste pine wood residue according to claim 1, wherein the epoxy resin glue in the step (3) is prepared by mixing epoxy resin and water at a mass ratio of 1-3.
4. The carbon sheet electrode manufactured by the method for manufacturing a waste pine residue-based carbon sheet electrode of any one of claims 1 to 3.
5. An electrochemical sewage treatment apparatus, wherein the carbon plate electrode according to claim 4 is used as a cathode electrode.
6. The electrochemical sewage treatment device according to claim 5, comprising a reaction tank (1), wherein a baffle (3) is fixedly arranged in the reaction tank (1), both sides of the baffle (3) are respectively provided with a magnetic generation electric roller (2) and a carbon plate electrode (5), the middle part of the baffle (3) is provided with a water flow channel, the magnetic generation electric roller (2) and the carbon plate electrode (5) are connected through a lead (4), the reaction tank (1) is provided with an aeration device, and both sides of the reaction tank (1) are respectively provided with a water inlet and a water outlet.
7. The electrochemical sewage treatment apparatus of claim 6 wherein the aeration device comprises a microporous aeration tray at the bottom of the reaction tank, the microporous aeration tray being in communication with the blower.
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